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Improved extraction method for tylosin

A technology of tylosin and co-solvent, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of high impurity content, difficult purification, and low product yield

Active Publication Date: 2009-10-28
荷本(北京)大药厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The experiment of the present invention shows: 1, when simply extracting tylosin with chloroform, the extraction rate is the highest, but the impurity content is also the most in the chloroform extract, which brings difficulties to purification, and the purification process tylosin The loss is more, and the product yield is lower than that of co-solvent extraction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1, extract tylosin (TL) from fermentation filtrate with butyl acetate (BA)

[0023] This extraction method is the tylosin extraction process used in factories at the present stage. The extraction process is as follows:

[0024] Fermentation filtrate, pH 6.21, titer 6500-6800 μg / ml, adjusted to pH 8.41 with 40% NaOH, added BA and stirred to extract TL. The amount of each extraction: fermentation filtrate / BA=100 / 30 (volume / volume, v / v)

[0025] Results: The residual potency of the aqueous phase after the first extraction: 1150μg / ml, the extraction rate of tylosin: 83.05%;

[0026] The residual potency of the aqueous phase after the second extraction: 521 μg / ml, the total extraction rate of the two extractions: 92.32%.

example 2

[0027] Example 2, extract tylosin (TL) with 3.85% chloroform (TT) / butyl acetate (BA)

[0028] (1) Fermentation filtrate used in experiments, titer 6500-6800 μg / ml, pH 6.21. Take 200ml fermentation filtrate, and use saturated Na 2 CO 3 Adjust the pH of the aqueous solution to 6.90-6.98, place it in a 35°C water bath, and raise the temperature of the fermentation filtrate to 30-33°C.

[0029] (2) Take it out at room temperature with stirring, and adjust the pH to 8.2-8.5.

[0030] (3) Pour into a 250ml separatory funnel, add 8ml TT / BA (3:1), mix well and let it stand for about 2 hours, separate completely, release the lower layer, then add 8ml TT / BA (3:1) to the upper layer Perform a secondary extraction.

[0031] (4) Combine the extracts from the lower layer twice, centrifuge, wash the precipitate with a small amount of TT, centrifuge, pour out the supernatant and combine with the centrifuged extract, and dehydrate with anhydrous sodium sulfate.

[0032] (5) Add 0.12g of tar...

example 3

[0038] Example 3, extract TL with 5.7% TT / BA (3: 1)

[0039] (1) Fermentation filtrate, pH 6.37, adjust pH to 6.98, put in 35°C water bath, raise the temperature of fermentation broth to 30°C.

[0040] (2) Take 200ml of fermented filtrate at 30°C and pH 6.98, mix with saturated Na 2 CO 3 The aqueous solution was adjusted to pH 8.44.

[0041] (3) Add 12ml TT / BA (3:1) to a 250ml separatory funnel, mix and extract thoroughly, let stand for 2.5 hours, completely separate layers, take 0.5ml upper layer, add 4.5ml water, and analyze by HPLC.

[0042] (4) The pH of the upper aqueous phase is 7.97, add 12ml TT / BA (3:1) for the second extraction.

[0043] (5) Take 200ml of new fermentation filtrate, adjust the pH to 6.9, heat the fermentation liquid at 35°C to 30°C (pH 6.70), and use saturated Na 2 CO 3 (about 5ml) to adjust the pH to 8.67, add the second extraction ester phase liquid in item (4) to carry out the first extraction of this batch (the second extraction solvent is app...

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Abstract

The invention relates to an improved extraction method for tylosin. The invention describes the process of using a cosolvent to extract the tylosin from tylosin fermentation filter liquid. The cosolvent comprises chloroform or methylene dichloride and ethyl acetate or butyl acetate or amyl acetic ester or isoamyl acetate or 4-methyl-2-pentanone or toluene. The method using the cosolvent to extract the the tylosin from the fermentation filter liquid has the advantages that the use quantity of the cosolvent is only 1-8% of the quantity of the fermentation filter liquid; the extraction rate is high and can reach 98.8%; and the cosolvent has a selective extraction function, the impurity content of extraction liquid is very little, product purification is convenient and the product purity is improved.

Description

technical field [0001] The invention relates to antibiotic refining technology. It specifically relates to the extraction technology of tylosin, which is a method for extracting tylosin from tylosin fermentation filtrate with co-solvent. Background technique [0002] Tylosin is a special antibiotic for livestock and poultry, which is a fermentation product of Streptomyces freundii. At present, liquid submerged fermentation is used at home and abroad. After the fermentation liquid is treated with a flocculant (such as aluminum sulfate or aluminum chloride), the fermentation filtrate is obtained through solid-liquid separation. The fermentation filtrate is subjected to liquid-liquid extraction with butyl acetate to obtain an ester phase liquid. , the tartaric acid or tylosin phosphate can be obtained by back-extracting, concentrating and spray-drying the ester phase liquid. [0003] Using butyl acetate to extract tylosin from the fermentation filtrate has the following two d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 王玉万潘真德戴晓曦
Owner 荷本(北京)大药厂有限公司
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